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管花肉苁蓉总苷提取纯化工艺及抗氧剂330合成研究
吴成
学位类型硕士
导师赵文军
2012-05
学位授予单位中国科学院研究生院
学位授予地点北京
学位专业有机化学
关键词管花肉苁蓉 稳定性 大孔树脂纯化 松果菊苷 苯乙醇苷
摘要研究发现新鲜植株体内存在的水解酶对苷类化合物,特别是苯乙醇苷类成分具有酶解和破坏作用,使后者含量减少,药材的药效降低。目前一般采用加热灭活酶的方法来抑制酶解和褐变。然而,除此之外,苯乙醇苷成分化学结构稳定性差,易发生酶解和化学水解,在加工和应用时苯乙醇苷损失严重。目前公开的技术只对前者进行了解决,而没有涉及加工过程或制剂应用时因化学环境变化导致的苯乙醇苷分解与氧化的问题。为了更好的开发该产品,本论文从以下五个方面对苯乙醇苷的提取和纯化进行了系统的研究。 首先,采用高效液相色谱法对管花肉苁蓉中苯乙醇苷类成分松果菊苷和毛蕊花糖苷进行了含量测定研究。通过采用kromasil色谱柱,以0.5%醋酸水为流动相A,以乙腈为流动相B,流速为0.9mL/min,检测波长310nm,柱温35℃,可以同时测定样品液中松果菊苷和毛蕊花糖苷含量。 然后,采用高效液相色谱法,测定在一定温度,不同pH值条件下样品液中松果菊苷和毛蕊花糖苷的浓度,发现在酸性条件下,松果菊苷和毛蕊花糖苷浓度较大;碱性条件下,松果菊苷和毛蕊花糖苷极易被分解破坏;在pH=3时,松果菊苷与毛蕊花糖苷浓度最大,也即最稳定。 其次,通过对7种大孔吸附树脂的静态吸附与解吸特性的研究,确定HPD-300树脂是一种理想的吸附剂,该树脂对管花肉苁蓉提取物中松果菊苷和毛蕊花糖苷的吸附量均较大,并且易解吸,适宜对肉苁蓉中苯乙醇苷进行提取分离。通过对HPD-300树脂的动态洗脱特性研究,确定上样后先用3-3.5BV的水洗脱除去部分杂质,然后用40%乙醇作为松果菊苷和毛蕊花糖苷的洗脱剂。 再次,以HPD-300大孔吸附树脂作为苯乙醇苷类分离纯化的介质,通过梯度洗脱,获得了良好的分离纯化效果。先用水洗脱除去大部分杂质,再用40%乙醇洗脱,最后用70%乙醇洗脱。放大工艺中40%乙醇洗脱液中松果菊苷和毛蕊花糖苷含量之和均超过85%,远远超过了国际市场关于肉苁蓉提取物的标准,且回收率也均在90%以上。各组分洗脱液经减压浓缩和干燥称重后,总重量和松果菊苷、毛蕊花糖苷重量均满足重量守恒。本实验研究结果为工业上苯乙醇苷类的富集和纯化提供了参考。 最后,以大孔吸附树脂HPD-300和YMC S-50 gel反相硅胶柱为分离纯化介质,用20%乙醇洗脱液多次洗脱,分别对松果菊苷和毛蕊花糖苷进行富集,制得较纯的样品。
其他摘要It is found that the hydrolytic enzyme in fresh Cistanche Tubulosa will hydrolyze and damage the glycosides, especially phenylethanol glycosides. So that the latter content decreased and the efficacy of the herbs reduced. Heating is commonly used to inhibit the enzymatic hydrolysis and browning now. However, besides that, the chemical constitution of phenylethanol glycosides has bad stability, and can be easily hydrolyzed. Resulting in great loss in the Processing and Applications. At present, the published papers mainly consider about the former, but not about the effect of chemical environment change will have on the phenylethanol glycosides. For better development of the product, this paper will systematically discuss the extraction and purification process of phenylethanol glycosides in five aspects. Firstly, A HPLC method was established for quantitative determination of PhGs including Echinacoside and Acteoside in Cistanche Tubulosa. The detected conditions are as follows:kromasil column, mobile phase A: 0.5% acetic acid, mobile phase B: Acetonitrile, flow rate: 0.9ml/min, detected wavelength:310nm, column temperature:30℃. By this method, both Echinacoside and Acteoside can be detected with good separability. Secondly, by HPLC, we could get the concentration of both Echinacoside and Acteoside in the sample in different PH but the same temperature. We find that the Echinacoside and Acteoside have a higher concentration in acid condition but will be easily degraded in alkaline condition. In PH3, Echinacoside and Acteoside have a highest concentration and also are most stable. Thirdly, seven kinds of macroporous resins were used to compare their absorption and desorption PhGs from Cistanche Tubulosa. HPD-300 resin was chosen to be better absorbent material and it possesses high absorption and desorption capacity. HPD-300 resin’s dynamic desorption experiment showed that most of the impurities can be wiped off eluted by 3-3.5BV water firstly and then eluted by 40% Ethanol. Finally, HPD-300 macroporous absorption resin was selected to isolate and purify phenylethanoid glycosides from Cistanche Tubulosa for its good isolation and purification effect. Most impurities can be get rid of through elution by water firstly, then eluted by 40% ethanol and lastly eluted by 70% ethanol. In amplification process, The content of Echinacoside and Acteoside attained in 40% ethanol was more than 80% every time, exceeding the standard in international market, and the recovery rates were more than 90%. Each eluent component was weighed and determined after decompressing concentration and vacuum dry. It’s found that the weight of Acteoside and Echinacoside and the total weight all meet the weight conservation. The study provided the reference for collecting and purification of phenylethanoid in industry. At last, we used HPD-300 macroporous resin and YMC 50μm ODS-A inverse silica gel as purification medium, eluented with 20% ethanol for many times respectively, for the enrichment of phenylethanol glycosides and acquiring the pure samples.
文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/4387
专题资源化学研究室
作者单位中国科学院新疆理化技术研究所
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GB/T 7714
吴成. 管花肉苁蓉总苷提取纯化工艺及抗氧剂330合成研究[D]. 北京. 中国科学院研究生院,2012.
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